CN103022489A - Carbon nano tube phosphate lithium-embedded cathode material with low specific surface area and preparation method thereof - Google Patents
Carbon nano tube phosphate lithium-embedded cathode material with low specific surface area and preparation method thereof Download PDFInfo
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- CN103022489A CN103022489A CN2012105843692A CN201210584369A CN103022489A CN 103022489 A CN103022489 A CN 103022489A CN 2012105843692 A CN2012105843692 A CN 2012105843692A CN 201210584369 A CN201210584369 A CN 201210584369A CN 103022489 A CN103022489 A CN 103022489A
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Abstract
The invention discloses a carbon nano tube in-situ composite olivine type phosphate lithium-embedded cathode material with a low specific surface area, belonging to the technical field of a lithium ion secondary battery cathode material. The cathode material is formed by a phosphate lithium-embedded compound and carbon. The invention further discloses a preparation method of the phosphate lithium-embedded cathode material. The olivine type phosphate lithium-embedded cathode material prepared by the preparation method disclosed by the invention is high in electric conductivity, good in high-rate performance, and low in low specific surface area, and has good pulping and coating machining performances.
Description
Technical field
The invention belongs to the lithium ion secondary battery anode material technical field, be specifically related to the compound phosphate of olivine type class of a kind of low specific surface area carbon nano-tube original position embedding lithium anode material and preparation method thereof.
Background technology
Phosphate of olivine type class lithium intercalation compound LiMxNyPO
4(M, N=Fe, Co, Mn, Ni, Cr, V, Nb, Mg, Zn, Cu, Ti, W; 1=x+y, x=0～1) owing to have safety, environmental protection, abundant raw material and memoryless property, make it become the first-selection of anode material for lithium-ion batteries of new generation; But himself conductance is lower, such as the electronic conductivity of LiFePO4 10
-9The m/s order of magnitude has limited its application.Therefore be necessary the modification of phosphate of olivine type class intercalation materials of li ions.Openly phosphate of olivine type class intercalation materials of li ions carbon coats or the compound patent of nano-sized carbon original position both at home and abroad, but the LiFePO4 specific area that this method obtains is too large, is unfavorable for slurrying and the coating of phosphate of olivine type class embedding lithium.And complex manufacturing is unfavorable for industrialization.
Patent 200910043208.0 discloses the method for adding the catalyst synthesizing iron lithium phosphate/nanometer carbon pipe composite materials such as Fe, Co, Ni in a kind of synthesis material, but the elemental metals particles such as the Fe in the method catalyst, Co, Ni finally can remain in the lithium iron phosphate positive material, cause self discharge of lithium iron phosphate battery.Propose to use the method for carbon-source gas synthesizing iron lithium phosphate/carbon nano tube compound material in the patent 201010130909.0.This method industrialization is difficulty relatively, can only use in tube furnace, and uniformity and batch stability can not guarantee.Patent 201010288610.8 discloses and has a kind ofly made LiFePO4 by liquid phase method first, then fully mixes the method for last sintering in solution with nanometer amorphous carbon.The covered effect of the amorphous nano-sized carbon of this method, batch stability have much room for improvement.Patent 201110397625.2 discloses catalyst such as adding Fe, Co, Ni in a kind of raw material and has used the method for carbon source gas synthesis lithium manganese phosphate/nanometer carbon pipe composite material, but the elemental metals particles such as the Fe in the method catalyst, Co, Ni finally can remain in the manganese-lithium phosphate anode material, cause the lithium manganese phosphate self-discharge of battery; Use carbon source gas so that this technology commercialization is relatively more difficult, can only use in tube furnace, uniformity and batch stability can not guarantee.
Summary of the invention
The object of the present invention is to provide the compound phosphate of olivine type class embedding lithium anode material of a kind of low specific surface area carbon nano-tube original position, it not only has the conductance height, and large high rate performance is excellent, and has lower specific area.
The present invention also aims to provide the preparation method of the compound phosphate of olivine type class embedding lithium anode material of a kind of low specific surface area carbon nano-tube original position, by in raw material, adding carbon nano-tube or scattered carbon nano tube paste, the compound phosphate of olivine type class intercalation materials of li ions of preparation low specific surface area carbon nano-tube original position.
A kind of low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material, this positive electrode is comprised of the component of following percentage by weight: phosphate lithium intercalation compound 94-99.8%, carbon 0.2-6%; Described phosphate lithium intercalation compound chemical formula is LiM
xN
yPO
4, M is Fe, Co, and Mn, Ni, Cr, V, Nb, Mg, Zn, Cu, Ti, a kind of among the W, N is Fe, Co, Mn, Ni, Cr, V, Nb, Mg, Zn, Cu, Ti, a kind of among the W, and 1=x+y, x=0～1.
The specific area of this positive electrode is 1-16m
2/ g.
The preparation method of above-mentioned low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material, carry out in accordance with the following steps:
(1) with Li source compound, metallic element source compound, P source compound Li in molar ratio: (M+N): P=(0.98～1.02): (0.98～1.02): 1 is dispersed or dissolved in the solvent of carbon nano tube paste, obtains solid content and be 10～60% slurry;
(2) grind, until the D90 of slurry less than 2um, stops to grind;
(3) drying, thing is uniformly mixed;
(4) homogeneous mixture with gained places inert gas, calcines 2-20 hour down in 600～1200 ℃ of temperature in rotary furnace or pusher furnace.
Described carbon nano tube paste is comprised of the component of following percentage by weight: suspended dispersed thickener 0.4-2%, and carbon nano-tube 2-6%, surplus is water or 1-METHYLPYRROLIDONE.
Described suspended dispersed thickener is one or more among xanthans, Arabic gum, gelatin, PEG, CMC, PVP, PVB, the PVA.
Described solvent is one or more in deionized water, acetone, ethanol, propyl alcohol, the isopropyl alcohol.
Described Li source compound is one or more in lithium hydroxide, lithium carbonate, lithium oxalate, lithium acetate, lithium dihydrogen phosphate, lithium nitrate, the lithium acetate; Described P source compound is one or more in the phosphate of phosphate, metal N of phosphoric acid, lithium dihydrogen phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, metal M; Described metallic element source compound be the carbonate that contains metallic element M and N, oxalates, acetate, oxide, citrate, phosphatic one or more.
Described inert gas is nitrogen or argon gas.
D90 is less than 1um for the described slurry particle size distribution of step (2).
Described drying is that spray drying or bipyramid vacuum rotating are dry.
Beneficial effect of the present invention: the phosphate of olivine type class embedding lithium anode material conductance that the present invention makes is high, and high rate capability is good, and specific area is low, has good slurrying and coating processing characteristics.
Specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
Embodiment 1
At first 360g carbon nano tube paste (carbon nano tube paste contains the 7.2g carbon nano-tube, 4.8g xanthans and 348gN-methyl pyrrolidone) is scattered in the 1717g ethanol; Then respectively with Li
2CO
3, FePO
4, MgO is lithium source, phosphorus source, source of iron and magnesium source, is scattered in the alcohol solvent of front carbon nanotubes Li in 1.0: 0.01: 0.99 the ratio of stoichiometric proportion of Li, Mg, Fe
2CO
3, FePO
4, MgO total consumption be 729g, obtain solid content and be 27% slurry; Be ground to D90 less than 0.8um after, carry out spray drying, thing is uniformly mixed; The powder body material of dry gained is placed rotary kiln, and logical nitrogen, makes oxygen content less than 100ppm, be warming up to 680 ℃ of constant temperature calcinings after 10 hours in the stove slow cooling to room temperature obtain the LiFe of black
0.99Mg
0.01PO
4Positive electrode.
It is 0.98% that the materials'use carbon and sulfur analytical instrument that example 1 is made records phosphorus content; Use the specific surface instrument to record just 6.2m of specific area
2/ g; The first charge-discharge capacity can reach 155mAh/g when carrying out the button cell sign, and 10C can reach 135mAh/g.
Adopt four-point method test LiFePO4 PET film pole piece resistivity:
The material preparation: LiFePO4, PVDF (Wu Yu chemistry) and NMP make and contain 35% LiFePO4, the electrode slurry of 5%PVDF.
The pole piece preparation is in the scraper for coating of PET film with 200um, 80 ℃ of oven dry; By the strip of sanction as the wide 1cm of long 8cm*, at 30MPa pressurize 1min, controlling material bed compacted density is 2.0-12.2g/cm take superior pole piece
3
Use precision DC electric current and voltage source test pole sheet resistor, calculate this pole piece specific insulation.
Adopting said method to record the made resistivity of example 1 can be less than 7ohm.cm, and the LiFePO4 resistivity that common common carbon coats is greater than 75ohm.cm.
Embodiment 2
At first 360g carbon nano-tube (carbon nano tube paste contains the 14.4g carbon nano-tube, 5.6g Arabic gum and 340g deionized water) is scattered in the 1717g deionized water; Then respectively with Li
2CO
3, manganese oxide, ammonium dihydrogen phosphate, niobium oxalate be lithium source, manganese source, phosphorus source and niobium source, is scattered in the deionized water solvent of front carbon nanotubes Li in 1.0: 0.7: 0.3 the ratio of stoichiometric proportion of Li, Mn, niobium, phosphorus
2CO
3, manganese oxide, ammonium dihydrogen phosphate, niobium oxalate total consumption be 891g, obtain solid content and be 32% slurry; Be ground to D90 less than 0.7um after, carry out spray drying, thing is uniformly mixed; The powder body material of dry gained is placed rotary kiln, and logical nitrogen, makes oxygen content less than 100ppm, be warming up to 800 ℃ of constant temperature calcinings after 12 hours in the stove slow cooling to room temperature obtain the Li Mn of black
0.7Nb
0.3PO
4Positive electrode.
It is 1.59% that the materials'use carbon and sulfur analytical instrument that example 2 is made records phosphorus content; Use the specific surface instrument to record just 7.2m of specific area
2/ g; The first charge-discharge capacity can reach 148mAh/g when carrying out the button cell sign, and 10C can reach 110mAh/g.
The PET film pole piece resistivity that adopts four-point method to test this material:
The material preparation: LiFePO4, PVDF (Wu Yu chemistry) and NMP make and contain 35% manganese phosphate niobium lithium, the electrode slurry of 5%PVDF.
Pole piece preparation: in the scraper for coating of PET film with 200um, 80 ℃ of oven dry; By the strip of sanction as the wide 1cm of long 8cm*, at 30MPa pressurize 1min, controlling material bed compacted density is 2.0-12.2g/cm take superior pole piece
3
Use precision DC electric current and voltage source test pole sheet resistor, calculate this pole piece specific insulation
Adopting said method to record the made resistivity of example 2 can be less than 20ohm.cm, and the lithium manganese phosphate resistivity that common common carbon coats is greater than 200ohm.cm.
Embodiment 3
At first 360g carbon nano-tube (carbon nano tube paste contains the 18g carbon nano-tube, 4gPEG and 338gN-methyl pyrrolidone) slurry is scattered in the 1600g isopropyl alcohol; Then respectively with Li
2CO
3, FePO
4, niobium oxalate is lithium source, phosphorus source, source of iron and niobium source, is scattered in the isopropanol solvent of front carbon nanotubes Li in 1.0: 0.9: 0.1 the ratio of stoichiometric proportion of Li, Fe, Nb
2CO
3, FePO
4, niobium oxalate total consumption be 813g, obtain solid content and be 30% slurry; Be ground to D90 less than 0.9um after, carry out spray drying, thing is uniformly mixed; The powder body material of dry gained is placed rotary kiln, and logical argon gas, makes oxygen content less than 100ppm, be warming up to 1000 ℃ of constant temperature calcinings after 8 hours in the stove slow cooling to room temperature obtain the LiFe of black
0.9Nb
0.1PO
4Positive electrode.
It is 2.16% that the materials'use carbon and sulfur analytical instrument that example 3 is made records phosphorus content; Use the specific surface instrument to record just 9.2m of specific area
2/ g; The first charge-discharge capacity can reach 160mAh/g when carrying out the button cell sign, and 10C can reach 140mAh/g.
Adopt four-point method test LiFePO4 PET film pole piece resistivity:
The material preparation: LiFePO4, PVDF (Wu Yu chemistry) and NMP make and contain 35% LiFePO4, the electrode slurry of 5%PVDF.
Pole piece preparation: in the scraper for coating of PET film with 200um, 80 ℃ of oven dry; By the strip of sanction as the wide 1cm of long 8cm*, at 30MPa pressurize 1min, controlling material bed compacted density is 2.0-12.2g/cm take superior pole piece
3
Use precision DC electric current and voltage source test pole sheet resistor, calculate this pole piece specific insulation adopt said method to record the made resistivity of example 3 can be less than 6ohm.cm, and the LiFePO4 resistivity that common common carbon coats is greater than 75ohm.cm.
Embodiment 4
At first 360g carbon nano tube paste (carbon nano tube paste contains the 21.6g carbon nano-tube, 4.4g gelatin and 334gN-methyl pyrrolidone) is scattered in the 1100g propyl alcohol; Then respectively with Li
2CO
3, FePO
4, nickel oxide is lithium source, phosphorus source, nickel source and source of iron, is scattered in the isopropanol solvent of front carbon nanotubes Li in 1.0: 0.8: 0.2 the ratio of stoichiometric proportion of Li, Fe, Ni
2CO
3, FePO
4, nickel oxide total consumption be 712g, obtain solid content and be 34% slurry; Be ground to D90 less than 0.7um after, carry out the bipyramid drying, thing is uniformly mixed; The powder body material of dry gained is placed rotary kiln, and logical argon gas, makes oxygen content less than 100ppm, be warming up to 600 ℃ of constant temperature calcinings after 20 hours in the stove slow cooling to room temperature obtain the Li Fe of black
0.8Ni
0.2P0
4Positive electrode.
It is 2.95% that the materials'use carbon and sulfur analytical instrument that example 4 is made records phosphorus content; Use the specific surface instrument to record just 8.2m of specific area
2/ g; The first charge-discharge capacity can reach 155mAh/g when carrying out the button cell sign, and 10C can reach 130mAh/g.
Adopt four-point method test LiFePO4 PET film pole piece resistivity:
The material preparation: LiFePO4, PVDF (Wu Yu chemistry) and NMP make and contain 35% LiFePO4, the electrode slurry of 5%PVDF.
Pole piece preparation: in the scraper for coating of PET film with 200um, 80 ℃ of oven dry; By the strip of sanction as the wide 1cm of long 8cm*, at 30MPa pressurize 1min, controlling material bed compacted density is 2.0-12.2g/cm take superior pole piece
3
Use precision DC electric current and voltage source test pole sheet resistor, calculate this pole piece specific insulation adopt said method to record the made resistivity of example 4 can be less than 7ohm.cm, and the LiFePO4 resistivity that common common carbon coats is greater than 75ohm.cm.
Claims (10)
1. a low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material is characterized in that this positive electrode is comprised of the component of following percentage by weight: phosphate lithium intercalation compound 94-99.8%, carbon 0.2-6%; Described phosphate lithium intercalation compound chemical formula is LiM
xN
yPO
4, M is Fe, Co, and Mn, Ni, Cr, V, Nb, Mg, Zn, Cu, Ti, a kind of among the W, N is Fe, Co, Mn, Ni, Cr, V, Nb, Mg, Zn, Cu, Ti, a kind of among the W, and 1=x+y, x=0～1.
2. described a kind of low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 1 is characterized in that the specific area of this positive electrode is 1-16m
2/ g.
3. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 1 is characterized in that, carries out in accordance with the following steps:
(1) with Li source compound, metallic element source compound, P source compound Li in molar ratio: (M+N): P=(0.98～1.02): (0.98～1.02): 1 is dispersed or dissolved in the solvent of carbon nano tube paste, obtains solid content and be 10～60% slurry;
(2) grind, until slurry particle size distribution D90 less than 2um, stops to grind;
(3) drying, thing is uniformly mixed;
(4) homogeneous mixture with gained places inert gas, calcines 2-20 hour down in 600～1200 ℃ of temperature in rotary furnace or pusher furnace.
4. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3, it is characterized in that, described carbon nano tube paste is comprised of the component of following percentage by weight: suspended dispersed thickener 0.4-2%, carbon nano-tube 2-6%, solvent are one or more in deionized water or 1-METHYLPYRROLIDONE, ethanol, acetone and the isopropyl alcohol.
5. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 4, it is characterized in that described suspended dispersed thickener is one or more among xanthans, Arabic gum, gelatin, PEG, CMC, PVP, PVB, the PVA.
6. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3 is characterized in that described solvent is one or more in deionized water, acetone, ethanol, propyl alcohol, the isopropyl alcohol.
7. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3, it is characterized in that described Li source compound is one or more in lithium hydroxide, lithium carbonate, lithium oxalate, lithium acetate, lithium dihydrogen phosphate, lithium nitrate, the lithium acetate; Described P source compound is one or more in the phosphate of phosphate, metal N of phosphoric acid, lithium dihydrogen phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, metal M; Described metallic element source compound be the carbonate that contains metallic element M and N, oxalates, acetate, oxide, citrate, phosphatic one or more.
8. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3 is characterized in that described inert gas is nitrogen or argon gas.
9. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3 is characterized in that D90 is less than 1um for the described slurry particle size distribution of step (2).
10. the preparation method of described low specific surface area carbon nano-tube phosphoric acid salt embedding lithium anode material according to claim 3 is characterized in that described drying is spray drying or bipyramid rotary vacuumize.
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Cited By (3)
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| CN103346314A (en) * | 2013-06-25 | 2013-10-09 | 河北工业大学 | Preparation method of lithium-ion battery anode material |
| CN108226641A (en) * | 2017-12-30 | 2018-06-29 | 湖北金泉新材料有限责任公司 | A kind of test method of anode material for lithium-ion batteries conductivity |
| CN112166094A (en) * | 2018-05-30 | 2021-01-01 | 魁北克电力公司 | Ceramics, method for the production thereof and use thereof |
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| CN103346314A (en) * | 2013-06-25 | 2013-10-09 | 河北工业大学 | Preparation method of lithium-ion battery anode material |
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| US11649190B2 (en) | 2018-05-30 | 2023-05-16 | Hydro-Quebec | Ceramics, methods for the production thereof and uses of same |
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Effective date of registration: 20200810 Address after: 212000 Qinglong mountain road, Zhenjiang New District, Jiangsu Province, No. 113 Patentee after: JIANGSU CNANO TECHNOLOGY Ltd. Address before: 100023 Beijing City, Daxing District economic and Technological Development Zone Branch 2 Street No. 9 B2-4 Patentee before: CNano Technology Ltd. |